AN  INVESTIGATION 


OF  A 

MODIFIED  BUNSEN  ICE  CALORIMETER 

BY 

NELLIE  FLORENCE  BATES 


THESIS 

FOR  THE 

DEGREE  OF  BACHELOR  OF  ARTS 

IN 

PHYSICS 


COLLEGE  OF  LIBERAL  ARTS  AND  SCIENCES 
UNIVERSITY  OF  ILLINOIS 


1922 


Digitized  by  the  Internet  Archive 
in  2015 


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https://archive.org/details/investigationofmOObate 


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TABLE  OF  COBTEITTS 


I.  Introduction 

1.  Inrpose  of  the  Investigat ion 

2.  Calorimetry 

a.  Black’s  Calorimeter 

h.  The  Calorimeter  of  Laplace  and  Lavoisier 
c.  Bunsen’s  Calorimeter 

3.  Previous  Investigations  with  Bunsen  Calorim.eters 

a . Bunsen  ’ s V/ork 

h.  Invest igat ion  of  C.  Y.  Boys 

c.  r/ork  of  J.  ViY  Ye  11  or 

II.  The  Present  Investigation 

1.  Filling  the  Calorimeter 

2.  Methods  of  Freezing 

a.  Calcium  Chloride  and  Ice 
h.  Evaporating  Ether 
c Ice  and  Sodium  Chloride 

3.  The  Results 

a.  ,7ith  the  Old  Calorim.eter 
h.  v7ith  the  iTew  Calorimeter 


III.  Conclusion 


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IirVSSTIGATIQIT  0^  A HQDI^IEI)  EUIISSIT  ICS  CALORD,''iE'’P.SR 

I.  lilTRODUC^CIOR 

1.  xtirpose  o^f  ^he  InYestigation.  The  piirpose  of  the  in- 
vestigation was  to  test  the  action  of  a modified  Eimsen  Ice  Cal- 
orimeter. Theory  shov/s  that  the  Bimsen  Calorimeter  is  prom.ising 
for  the  determination  of  specific  lieats,  hut  the  results  of  ex- 
periments are  disappoint ing , hut  it  appears  that  the  instrument 
has  unexpected  defects.  It  was  thought  uliut  the  m.odified  calor- 
imeter might  overcome  one  of  these  defects. 

2.  Calorimetry*  Galorim.etry  is  the  scientific  name  for 
the  measurement  of  heat.  Tliere  are  several  different  m.ethods 
used: --method  of  mixtures,  m.ethod  of  cooling,  method  of  condensa- 
tion, energ:"  methods  (m.echanical  and  electrical)  , and  the  method 
of  fusion.  The  Eunsen  Ice  Calorimeter  belongs  to  the  last  class. 
The  earlier  forms  of  the  ice  calorimeter  were  those  of  Elach  and 
of  Laplace  and  Lavoisier. 

a.  Blach^  s Calorimeter.  Black’s  Calorimeter  consisted  of 
a block  of  ice  'with  a hole  m.elted  out  of  the  center.  An  object 
7/hose  specific  heat  was  sought,  was  heated  to  steam  tem.perature , 
inserted  in  this  cavity,  and  another  cake  of  ice  v/as  put  over 
the  top  for  a cover,  v/hen  the  object  had  come  to  ice  temperature, 
it  v/as  lifted  from,  the  cavity  and  the  ice  which  had  melted  was 
absorbed  by  a weighed  cloth  which  was  re-v/eighed  in  order  to  ob- 
tain the  weight  of  the  ice  m.elted. 

''"Encyclopedia  Erittanica,  11th  Ed.  Vol.V.,  page  52 


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imeter consisted  of  a small  vessel  placed  inside  o:^  a larger 
vessel  filled  .vi  th.  ice.  .Then  the  hot  body  was  placed  in  the 
inner  vessel,  some  of  the  ice  was  melted  end  this  was  drawn  o’'f 
at  the  bottom  and  weighed. 


A considere.ble  error  is  made  in  me asnr event s with  these 
calorimeters  because  of  the  difficultj;^  in  deteim'ining  exactly 
the  amount  of  ice  melted.  In  the  Black  C-a,lorimeter , the  manipu- 
lation with  the  cloth  is  lilcelv  to  melt  more  ice,  while  in  the 
Laplace  and  Lavoisier  instruivent , the  Y/ater  clings  to  the  ice, 
due  to  surface  tension.  ?he  Bunsen  Calorimeter  overcomes  this 
imcertainty  by  m.easuring  the  volume  melted  instead  of  the  weight, 
c.  Bunsen’s  Calorimeter.  The  Bunsen  Ice  Calorimeter 


consists  of  a large  test  tube 
glass  cylinder  'Yith  a capillar: 


, which  is  enclosed  in  a large 
tube  extending  from  the  bottom 
of  it  up  tiie  side.  The  inter- 
vening spfctce  between  these  tubes 
is  filled  T/ith  p''.ne  air. -free 
v/ater,  and  mercury.  Som.e  of  the 
water  around  the  tube  is  frozen 
and  since  ice  occupies  more  vol- 
ume than  water,  some  of  the  mer- 
cury is  pushed  out  into  the  side 


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graduated  tube  II.  v/hen  the  substance  whose  S]:ecific  heat  is  be- 
ing measured,  is  placed  in  T,  som;e  of  the  ice  is  m.elted  and  the 
mercury  recedes.  In  order  to  interuret  the  indications  of  the 


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ins t riii'ae nl: , a Imown  mass  of  v/ater,  m.  at  a definite  temperature, 
6,  may  "be  introduced  into  tlie  tube  T.  In  fillin{j  to  0®  C.,  this 
gives  out  a quantity  of  heat  m0,  and  in  consequence  of  the  melt- 
ing of  the  ice,  the  mercury  in  the  tube  H recedes  through  n div- 
isions of  the  scale,  fhis  gives  the  relation  between  the  quan- 
titj?"  of  heat  supplied  in  an.v^  e:q:ieriment  in  the  tube,  f,  and  the 
corresponding  recession  of  the  mercury  along  the  sca.le  H,  for 
if  q is  the  heat  corresponding  to  each  division,  we  have 

m0  - nq. 

In  determining  the  specific  heat  of  any  substance,  a fragment 
of  it  at  room  temperature  is  immersed  in  the  v/ater  in  the  tube  ?. 
More  ice  is  melted  ajid  the  mercury  recedes  n’  divisions  of  the 
scale,  the  whole  heat  given  up  by  the  body  in  cooling  to  zero  is 
nVq.  Then,  if  m'  be  the  mass  of  the  body  and  0’  its  original 
tem.perature , its  specific  heat  is  given  by  the  equation, 

m' s0 ’ = n' q 
hence  s 

m'n0^ 

This  all  sounds  very  well  until  it  is  tried --then  rnnny 
difficulties  a.re  encountered.  In  the  first  palace,  it  was  sug- 
gested and  later  proved,  tliat  a small  pocket  of  ice  was  melted 
right  around  the  glass  tube,  I,  bj'-  the  lie  at  given  up  by  the  v;ater 
and  the  substance  a,nd  that  the  ice  was  not  raelted  through.  If 
this  were  the  case,  the  volume  \70uld  not  be  changed  at  all  and 
the  m.erciiry  in  H would  not  be  affected. 

fhe  purpose  of  the  invest igat ion  was  to  try  to  overcom.e 
this  objection.  A new  calorimeter  was  ordered  m.ade  which  had 
small  platinum  v/ires  fused  in  the  tube  ? and  extending  out  into 


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the  ’/rater  through  tiie  ice.  -rhen  any  heat  in  the  tube  'V  would  he 
conducted  alo2ig  the  j'latinum  wires  and  would  ir.elt  the  ice  around 

them thus  alwa'^s  '^e^,ting  through  to  the 

water  and  ca,using  the  mercur'^  to  recede.  M- 
so,  it  seems  lihel"  that  the  ice  Y/oiild  form, 
around  the  v/ires  due  to  the  conduction  of 
the  heat  along  them  niore  ranidly  than  else- 


5.  Irevious  Invest igations  Jl^th  lims en  Calorimeters . 
a.  Bun_senh  fo^.  Hohert  ..'illiam  von  Bunsen  invented  his 
ice  calorimeter  at  rieidelterg  fniversitv  in  1870.  It  was  con- 
structed much  lilze  the  calorimeter  descrihed  above.  Ihe  cooling 
was  accomplished  by  passing  cooled  alcohol  tlirough  the  tube  1. 

He  foiuid  that  the  air  freed  water  inside  liad  to  be  cooled  far 
below  QO  C.  before  freezing  began;  the  water  froze  suddenly  and 
was  allov/ed  to  continue  freezing  until  a cy'  inder  of  tliiclmess 
from  six  to  ten  millim.eter'’  was  formed  around  the  inside  tube. 

The  ins-'-'uiment  was  '.‘n  pure  snow  which  was  changed  twice 

daily  and  the  tempoT*'^ t\ire  of  the  room  was  l.ept  from.  5*^  C,  to  6^  G. 
He  let  the  instrurr.ent  staiai  a da."  or  two  until  conditions  should 


become  steady  before  actually  perform.ing  his  experim:ent  . He 
found  that  the  water  ./as  so  cooled  before  freezing  began  ■■hat  it 
’would  continue  to  freeze  '.'or  about  114  hours,  for  his  calcula- 
tions he  r.sed  the  formula: 


T «=  number  o'f  scaH.e 

divisions 

3 -,%Gt  ■ 

“ am 0 Vint  of  heat 

given  up  bv  one 

gram  of  v/ater  ’/ 

/h  en  c 0 0 le  d f r om; 

v/eight  of  substance 

10  C.  to  QO  C. 

tested 

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^investigation  oi  C,  Y.  Boys.  Professor  Bogs  suggested 
that  a protecting  cover  of  glass  he  provided.  If  the  vihole  sur- 
face of  the  glass  is  in  contact  ':.'ith  the  outer  snow,  the  conduc- 
tivity of  heat  will  he  very  great  if  there  is  a slight  difference 
of  temperature  hetv.'een  the  two  sides,  fhe  amount  of  heat  pass- 
ing through  the  walls  of  the  ir^trujj’ent  depends  on  the  difference 
of  temperature  and  the  conductivity,  end  if  both  of  these  factors 
can  he  minimized,  so  much  the  better.  He  suggested  that  the 
instruirent  lie  in  the  glass  cover  and  that  the  tv/o  tubes  he  sup- 
ported by  a thin  India  rubber  cork  fitted  into  the  upper  end  of 
the  glass  cover.  A.  third  hole  in  the  cork  carried  a glass  tube 
v/ith  a stop-cock.  If  there  wa.s  any  hurry  to  cool  the  instru- 
ment, ice-cold  vvater  was  poured  in  upon  the  ice  so  as  to  reach 
above  the  lower  end  of  the  protecting  tiibe,  and  the  stop-cock 
opened  and  the  air  dravm  out  if  necessary  until  tlie  water  reached 
the  cork.  This  water  may  be  changed.  M'ter  the  v/ater  inside  the 
calorimeter  was  frozen,  the  water  on  the  outside  was  dravm  out 
and  the  instrunient  was  ready  for  use.  It  was  foiuid  that  this 
cover  v/as  a decided  im.provement . 

3.  \J or k of  J . ;7 . Me  1 1 or  . * Professor  Fein.or's  contribution 
was  a new  method  of  filling  the  calorimeter.  He  says,  "The  com- 
plete separation  of  dissolved  air  fromi  the  water  used  in  mailing 
the  'ice  kernel'  is  necessary  for  accurate  results.  At  any  time 
the  separation  of  air  from  water  so  that  the  latter  v/ill  give 
the  characteristic  'click'  is  a difficult  ma,tter,  v/hile  the 
filling  of  the  calorim.eter  with  such  water  is  a still  more  tedious 

*J.  kellor  "Hotes  on  Bunsen's  Ice  Calorimeter”,  Journal  of 

Physical  Chemistry,  Vol.  4,  pp.  135-156 


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operation.  rile  end  oi  the  liehig's  condenser  (I),  is  fitted  to 
the  side  necic  of  an  ordinary  liter  distilling  flash  and  the  other 
end-  is  connected  to  a water  air-pump.  ?he  flash  (h)  is  about 
half  filled  rrith  distilled  water,  and  the  outer  chamber  of  the 
calorimeter  is  about  one  third  filled  with  distilled  -.7ater.  A 
tube  dipping  almost  to  the  bottom,  is  fitted  into  the  nech  of  the 
distilling  flash  and  also  into  the  opening  of  the  side  tube  of 
the  calorimeter.  -he  pmnp  is  set  in  action,  and  the  water  in  the 
calorimeter  is  hea/ted  by  a Bunsen  flar.B  with  a sheet  of  a.sbestos 
placed  under  it.  fhe  ilash  is  healed  owe:?  a sand  bath  until  its 
coni:ent.s  give  the  characteristic  hamm.ering  when  shahen.  fhe  lamp 
is  then  rem.oved  fro]-  luider  the  calorimeter  and  the  latter  will 
verv  soon  be  filled  with  air-free  w/ater.  fhe  troublesomie  bumping 
of  the  w/ater  boiling  luider  reduced  pressiire  is  considerab].','  modi- 
fied by  the  tube  dipping  under  the  water  in  the  flash. 


/f 


port  ant  pa,rt  of  the  experiment  was  to 


^ ^1^1  _Calg)  rij!ie_^t  e r . ?r ob  ab ly 

the  m.ost  difficult  and  the  m.ost  im- 


fill the  calorimeter  with  uiu'e  air- 


'vee  water 


It  w/as  found  best  to 


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heat  the  calorimeter  cautiously  to  drive  out  some  of  the  air,  then 
to  put  the  open  end  (0)  under  some  pure  distilled,  boiled  water. 

As  the  air  cooled  and  contracted,  some  of  the  water  was  dravm  over 
into  the  space  (S).  If  this  water  were  boiled  vigorously  ?/ith  a 
Eimsen  flame  (B) , the  air  in  fS)  was  driven  out  and  the  space  was 
filled  v;ith  vapor.  .’Aien  the  flame  was  reuioved,  this  vapor  con- 
densed and  Y/ater  was  syphoned  over  into  fS)  with  a great  rush 
filling  the  space  fS).  fhere  was  always  a small  bubble  of  vapor 
remaining,  but  if  the  water  were  allowed  to  cool,  this  contracted 
to  a very  sm.all  space  and  if  the  tube  were  turned  upright  very 
carefully,  it  ascended  the  small  side  tube.  ITercury  was  then 
poured  into  the  side  tube  and  poked  down  with  an  iron  wire.  This 
was  very  clujnsy  arid  took  a ver-'^  long  time  ‘because  the  water  had 
to  }Dush  up  past  the  mercury  before  the  mercury  could  get  dovm. 
Later,  a quicker  and  m.ore  satisfactory  m.ethod  was  found  by  which 
m.ercury  was  pouned  in  to  about  one -tenth  of  the  volume  fS)  after 
the  first  step  in  filling  (when  only  a little  water  \7as  in  fS). 

The  m.ercury  did  not  interfere  in  the  least  with  the  rest  of  the 
filling.  ./hen  the  water  had  cooled  and  the  vapor  bubble  removed, 
the  side  tube  v/as  filled  with  miercury  also  and  the  calorimeter  was 
ready  for  use . 

Blethods  of  freezing.  The  calorimeter  which  rested  on 
a large  cork  and  som.e  soft  wax  to  prevent  breakage,  was  placed  in 
a mntal  box  made  specially  for  the  piirpose  and  was  packed  in  pure 
shaved  ice.  A rubber  cork  fitted  in  the  top  of  the  side  tube 
carried  a capillary  glass  tube  which  was  bent  a^id  extended  about  a 
mieter  along  a scale.  As  the  water  froze,  the  riBrcury  was  pushed 
from  the  side  tube  out  along  the  capillary  tube. 


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- 8 - 

a.  Calciap  Chloride  aiad  Ice.  The  first  freezing  mixture 
tried  v/as  calcium  chloride  and  shaved  ice  in  tlie  ratio  of  three 
parts  ice  to  four  parts  calcium  chloride  by  vzeight  . A low  temper- 
ature k>ias  not  obtained  v/ith  this  because  the  calcium  chloride  v/as 
not  the  right  sort — crystalline  is  the  hind  to  be  U3ed--iind  not 
large  enough  q^uantities  were  mixed  at  one  time.  Later  crystalline 
chloride  was  ground  to  a powder  and  mixed  with  ice.  It  v;as  fornd 
that  a temiperature  of  a 0.  could  be  obtained  in  this  way,  but 
this  was  inconvenient  to  use  since  the  calcium,  chloride  did  not 
dissolve,  but  sank  to  the  bottom  of  the  tube  and  could  not  be 
syphoned  out.  It  v/as  necessar,y  to  turn  the  calorimeter  upside 
dov/n  to  get  rid  of  this. 

b.  Evaporating  Ether.  A much  miore  convenient  method  was 
to  vv.t  ether  in  the  inner  tube  (T)  and  connect  it  to  an  aspirator, 
so  that  air  v;as  bubbled  through,  the  ether  thus  causing  a ra,pid 
evaporation  arfL  cooling.  This  did  not  prove  successful.  The  fail- 
ure was  probably/  due  to  the  fact  that  the  v/arm  air  drawn  through 
the  aspirator  heated  the  calorimeter  about  as  fast  as  it  v/as  cooled. 
Later,  the  freezing  was  started  v/ith  the  calcium  chloride  mixture 
and.  then  it  was  attempted  to  build  out  the  ice  with  the  ether, 

but  it  was  found  that  the  ice  was  only  melted. 

Ice  nnd  Sodium  Chloride.  One  da,y,  by  chance,  it  was 
found  that  if  three  parts  snow  to  one  ]part  sodium  chloride  were 
mvixed  together  in  large  enough  quantities,  a temperature  of  a -18° 

C.  could  be  obtained.  This  mixture  froze  the  water  in  the  calor- 
iwieter  ver:'  nicely  in  a short  time  and  was  also  convenient  to  clean 
out  after  the  freezing  was  accomplished.  If  the  calorim.eter  v/ere 
rinsed  with  v/ater  at  about  0°  C.,  and  thus  syphoned  out,  the 


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Calorimeter  vroald  be  clean  and  ready  for  use. 

Result 5 . Tlie  calorimeter  was  then  used  to  find  the 
specific  heat  of  aluminum.  First  the  instrument  v/as  calibrated  by 
pouring  a 'weighed  am.ount  of  water  into  it  and  noting  how  many  centi- 
m.eters  the  mercury  receded.  Then  a small  alum.inum  coil  was  placed 
in  the  tube  so  tlat  it  was  jiist  'covered  with  water.  Again  the  num.*- 
ber  of  centimeters  that  the  m.ercury  receded  was  observed.  Then 
from  the  formula 

mn’  0 
S = m’nQ' 

mentioned  above,  the  specific  heat  of  aluminum,  was  calculated. 

DATA 


.L' 

'irst  Trial 

Second 

Third 

Weight  of 

v^ater 

3.1321  grfls. 

5.6565 

3.125 

V/ eight  of 

aluminum 

5.767 

3 . 7941 

3.7941 

Divisions 

of  recession  for  water 

7.3  cm. 

4.2 

1.8 

Divisions 

of  recession  for  al. 

1.6 

1.9 

1.2 

Cliange  of 

tem.perature  of  'water 

23.10  C. 

24.5 

22,8 

Change  of 

temperature  of  al. 

23.50 

22.6 

22.8 

Calculated  specific  heat 

.182 

.63 

.05 

These  preliminary  results  were  not  good  since  the  accepted  value 
for  the  specific  heat  of  aluminum  is  .2143.  The  same  experiment 
was  repeated  several  tim.es  and  without  concordant  results,  \7hen 
an  imrestigation  v/as  made  to  see  what  was  the  trouble,  it  was  found 
each  time  that  just  as  was  expected,  a srr.all  pocket  of  water  was 
enclosed  bet'vveen  the  wall  of  the  tube  and  the  ice  aroimd  it  and 
that  the  ice  was  not  melted  through.  Of  cou3?se  this  being  the  case, 
no  reliable,  results  could  be  obtained. 

Fig.  5 is  a photograph  of  the  calorim.eter  after  water  is 
poured  to  i^ielt  the  ice.  A pocket  is  shown  as  suspected  between 


^ a 


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tlie  glass -and  the  outer  coating  of  ice  that  would  prevent  a change 
in  volume  and  a movement  of  the  mercury  column. 

The  investigation  originall.y  planned  was  not  completed. 

A calorimeter  ?/ith  platinum  wires  was  secured  and  tried,  hut  it 
Proved  to  he  defective  in  that  the  sealing  between  the  wires  and 
the  glass  was  not  perfect  so  that  water  leaked  tlirough.  The  in- 
strument maker  was  unahle  to  complete  a nev/  calorimeter  in  time 
for  this  investigation. 

III.  OOIJOLUSIOiT 

Tlie  results  obtained  give  promise  of  showing  the  effect 
sought,  nam.ely  that  the  ice  melts  in  a pocket  aromid  the  inner 
tube  so  that  the  outer  coating  of  ice  prevents  a change  in  volume 
of  the  enclosed  water,  and  the  mercury  column  does  not  move. 

Acloiowledgments  are  due  to  Professor  P.  R.  ilatson  who 
offered  the  suggestion  for  the  investigation  and  gave  much  en- 
couragement and  helpfullness  to  the  investigators,  and  to  Miss 
Vera  V.  Bassett,  my  partner  in  the  experiment. 


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BIBIIOGRimr/ 


1.  C.  V.  Bojs,  "On  an.  Mdition  to  Bunsen’s  Ice  Calorimeter", 
Philosophical  IiSagazine,  Vol.  24,  Year  1887,  page  214. 


2.  R.  Bunsen,  "The  Ice  Calorimeter",  Philosophical  Magazine, 
1871,  Yol.  XL.,  page  161.  ^ 

(Translated  hy  Yrancis  Jones  from  Poggendori’s  .‘''innalen, 

ilo.  9,  1870) 


2.  H.  S.  Callendar,  "Calorimetry",  Snc3rclopaedia  Brittanica, 
Eleventh  Edition,  Yol.  5.  pages  SC-SO. 


4.  J.  Y.  Mellor,  "ITotes  on  Bunsen’s  ice  Calorimeter",  J ournal 
of  Physical  Chemistry,  Yol.  4,  page  135-136,  Peh.,  1900. 


5.  Preston,  "Theory  of  Heat” 


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< ^ '■  , ■ >''-:rtM  '^w  * 4M  , ■‘¥^'■1  .#1 


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